CN1343738A - Chemically cross-linked millipore polyethene material and its preparing process - Google Patents
Chemically cross-linked millipore polyethene material and its preparing process Download PDFInfo
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Abstract
A millipore polyethylene material is prepared from polyethylene resni as basic component, foaming agent, cross-linking agent, nucleator, and liquid assistant through mixing, chemical cross-linking and chemical foaming. Its advantages include apparatus density of 20-100 kg/cu.m, thickness of 1-10 mm, high mechanical strength and thermal insulation, controllable uniform pores, and high size stability.
Description
The present invention relates to millipore polyethene material and preparation method thereof, further, the present invention relates to millipore polyethene material of chemical crosslink technique preparation and preparation method thereof.
Millipore polyethene material has advantages such as water-fast moisture resistance, heat-insulating sound-insulating, wear-resisting, chemical-resistant resistance.Millipore polyethene material is an obturator-type, because its crystallinity and apparent density descend, this kind material is generally semihard, and air can infiltrate abscess.When loading, some air can be overflowed from abscess, and after the loading cancellation, air can spread back abscess again.Thereby this kind poromerics shows excellent anti-strike, endergonic characteristic.Because the polythylene resin melting range is very narrow, near melt temperature, its viscosity reduces very fast when raising.So just cause foaming instability, bubble easily to break easily.So at present the employing carried out crosslinked method with the method or the employing of polyethylene and other resin alloy to matrix resin more, the melt strength that improves foamed substrate also obtains suitable melt flow viscosity, improves the degree of stability of foaming process thus.But this method can only play limited effect for the control of foamed stability, so be difficult for making high foamability and the special stabilized uniform foam material of abscess, general thin, the small-sized foaming product of production that only is fit to.As the flat 1-275640 of Japanese Patent, with the blend of new LDPE (film grade) and ethene, alpha-olefin copolymer through chemically crosslinked and foaming and polyethylene foam-material.The apparent density of its material is 36Kg/m
3, tensile strength is 0.45MPa, elongation at break is 235%.The polyethylene foamed material of this patent be thickness be the thin slice of 3mm, do not relate to for the wide cut foam sheet thicker, high foamability, that dimensional stability is had relatively high expectations.
The purpose of this invention is to provide a kind of is the millipore polyethene material of main matrix resin with new LDPE (film grade).Its expansion ratio height, abscess homogeneous and controllable, dimensional stability are good, are fit to make thicker, large-scale foaming product.And the apparent density of this millipore polyethene material and thermal conductivity is low, mechanical property is excellent.
Another object of the present invention provides the preparation method of described millipore polyethene material.
Millipore polyethene material of the present invention is achieved in that
Millipore polyethene material matrix resin of the present invention comprises the blend of new LDPE (film grade) or new LDPE (film grade) and other polymkeric substance, as the blend of new LDPE (film grade) and following at least a material: high density polyethylene(HDPE), linear low density of polyethylene, polyhutadiene, ethylene-ethyl acetate copolymer, second third copolymer or ethylene-propylene terpolymer.The weight ratio that new LDPE (film grade) accounts for blend in the blend of new LDPE (film grade) and other polymkeric substance is (60～95): 100, be preferably (80～90): 100.
This kind millipore polyethene material is the obturator-type structure, and abscess homogeneous and controllable, expansion ratio height, dimensional stability are good.This poromerics pore size is 0.20～0.60mm.The apparent density of material is 20～100kg/m
3, be preferably: 25～35kg/m
3The area density of material is 0.1～0.4kg/m
2The thickness of this kind foam material can reach 1～10mm, is preferably 4～10mm.Its tensile strength 〉=0.3MPa, elongation at break 〉=100%, the thermal conductivity to air is 0.03～0.04W/m.K at normal temperatures.This kind material is fit to do large-scale foaming product, is fit to foam sheet, especially the wide cut foam sheet of various width, and its width can reach more than the 0.5m.
This millipore polyethene material can be used for the wrapping material of the door lining that protects curtain, floating matter, automobile, ceiling liner and the fragile article of agricultural booth, the shockproof energy-absorbing materials such as shock resistant packaging material of guided missile.
Millipore polyethene material of the present invention prepares by chemical method is crosslinked.The whipping agent that has used high umber in foaming process is to improve expansion ratio, because the foaming process of high umber whipping agent is wayward, so added the auxiliary agent that foaming process is played control, stabilization simultaneously, foam to guarantee to stablize, thereby obtain high foamability and the uniform poromerics of abscess.So that present method is well suited for is thicker, the foaming of massive article.
This preparation method may further comprise the steps:
(1) processing aids such as the same whipping agent of matrix resin, linking agent, nucleator and liquid adjuvants is mixed;
(2) with mixture blend, crosslinked moulding then, blending temperature is generally 150～170 ℃;
(3) with the foaming of section bar thermostatically heating, be generally heat-up time 3～15 minutes, blowing temperature is generally 200～230 ℃.
Polyethylene matrix resin comprises the blend of new LDPE (film grade) or new LDPE (film grade) and other polymkeric substance in this method, as the blend of new LDPE (film grade) and following at least a material: high density polyethylene(HDPE), linear low density of polyethylene, polyhutadiene, ethene-vinyl acetate copolymer, second third copolymer or ethylene-propylene terpolymer.The weight ratio that new LDPE (film grade) accounts for blend in the blend of new LDPE (film grade) is (60～95): 100, be preferably (80～90): 100.
For the polyethylene matrix resin of foam material, the melt-flow viscosity of resin itself and melt strength are to resin expanded relevant, and aforesaid resin material preferably is chosen in the high resin of melt strength under the melt-flow viscosity that can process.
Adopt chemical crosslink technique to carry out crosslinked in the cross-linking step of present method to matrix resin.Linking agent selects for use decomposition temperature at 110～170 ℃ superoxide, is preferably dicumyl peroxide or benzoyl peroxide.The consumption of linking agent is suitable, and consumption can make degree of crosslinking too low very little, does not have the crosslinked corresponding effect of bringing; Can cause excessively crosslinked again and the influence foaming causes unit weight too high if consumption is too high.Be that the consumption of 100 linking agents is 0.3～7 in the matrix resin parts by weight in present method, be preferably 0.5～5.
Whipping agent is selected the solid state chemistry whipping agent for use in the processing aid of present method, is preferably azo-compound, wherein is preferably Cellmic C 121 or Diisopropyl azodicarboxylate.The consumption of whipping agent can have influence on bubble quantity and bubble, size and further influence the generation of bubble.For the poromerics present method that obtains high foamability is used high umber whipping agent, its consumption is 100 to count 10～28 with the matrix resin parts by weight, is preferably 15～22.
Be to use the whipping agent of high umber to prepare the poromerics of high foamability in present method and the prior art key distinction, added the auxiliary agent that helps stable foaming simultaneously, be nucleator and liquid adjuvants, they are even, stable for forming in the foaming process, fine and close abscess has played important effect, is key point of the present invention.
When making millipore polyethene material, the nucleator role is extremely important to foaming process as the effect of zeolite in boiling liquid.Say that accurately nucleator forms focus air bubble growth point when foaming, just can form bubble at air bubble growth point when whipping agent decomposes, nucleator plays very important effect for the uniform distribution and the stable growth of abscess.In addition, can control the size of abscess by the consumption of regulating nucleator.Nucleator is generally thin solid particulate, and flap or wax are also arranged.Nucleator comprises the solid particulate of inorganic salts and metal oxide in present method, can be selected from silicon-dioxide, talcum powder, lime carbonate, zinc oxide or magnesium oxide etc.The too high weighting agent that then becomes of nucleator consumption has not had the effect of focus on the contrary, so its consumption is 100 to count 0.2～2 with the matrix resin parts by weight, is preferably 0.5～1.5.
In the course of processing of millipore polyethene material, liquid adjuvants has played the lubricated effect that reaches abscess adjustment when foaming in extrusion, and its adding helps extruding of foam material, also helps to form abscess uniform and stable, controllable size.In addition, when matrix resin and processing aid uniform mixing, add liquid adjuvants processing aid is evenly adhered on the matrix resin, guaranteed that blended is even, reduced the consumption of auxiliary agent.At this liquid adjuvants is low molecule straight chain hydrocarbon of liquid or the low molecule silicoorganic compound of liquid, is preferably white oil, whiteruss or silicone oil.Liquid adjuvants adds and not to have effect very little, then is unfavorable for processing too much, so its consumption is 100 to count 0.5～10 with the matrix resin parts by weight, is preferably 1～5.
The prescription of matrix resin and processing aid is 100 to count with the matrix resin parts by weight:
Matrix resin 100
Whipping agent 10～28
Linking agent 0.3～7
Nucleator 0.2～2
Liquid adjuvants 0.5～10
Screening formulation is 100 to count with the matrix resin parts by weight:
Matrix resin 100
Whipping agent 15～22
Linking agent 0.5～5
Nucleator 0.5～1.5
Liquid adjuvants 1～5
In preparation process, according to the processing needs, processing aid can also be selected other some plastic working usual auxiliaries for use, as pigment, fire retardant etc.The fire retardant of foam material should notice that the kind of the fire retardant that uses and umber can not have influence on foaming in use.So can comprise halogen flame, antimonous oxide and phosphonium flame retardant etc. at this employed fire retardant.Phosphonium flame retardant comprises: trimethyl phosphite 99, triphenylphosphate, tricresyl phosphate (2,3-two chloropropyls) ester, tricresyl phosphate toluene bromide ester, red phosphorus, Tetrakis hydroxymethyl phosphonium chloride etc. are preferably triphenylphosphate.The consumption of phosphonium flame retardant is 100 to count 2～6 with the matrix resin parts by weight.Halogen flame comprises: decabromodiphenyl oxide, octa-BDE, hexabromobenzene, clorafin, perchloro-penta cyclodecane etc. are preferably decabromodiphenyl oxide.Antimonous oxide can cooperate the halogen flame use also can use separately.The total consumption of halogen flame and antimonous oxide is 100 to count 3～25 with the matrix resin parts by weight, is preferably 8～15.Amount ratio is 1: 3～1: 2 when antimonous oxide and halogen flame use jointly.
The uniform mixing of matrix resin and processing aid generally carries out at normal temperatures in present method.The equipment that uses is general raw material mixing equipment, as high-speed mixer, common kneader or tumbler mixer etc.
Present method in the step of blended cross linking, use blending equipment as the general blending equipment in the rubber and plastic processing industry, can comprise mill, Banbury mixer, single screw extrusion machine or twin screw extruder etc.
The moulding of material can comprise general plastic shaping methods such as compression molding method, injection molding method or extrusion moulding.
The equipment that uses in section bar foamable step is that general thermostatically heating equipment comprises hot drying tunnel, oven heat etc.
Present method is applicable to the kinds of processes of polyethylene foam, as technologies such as extrusion foaming, moulded from foam, injection foaming or the foaming of expandability pellet.The Fig. 2 in the accompanying drawing is seen in the flow process signal of these technologies.
The millipore polyethene material mean pore size of present method gained is 0.20～0.60mm, the expansion ratio height, and apparent density is 20～100Kg/m
3, area density is 0.1～0.4kg/m
2, material thickness is 1～10mm.This kind material mechanical performance is good, heat-proof quality good, dimensional stability is good, its tensile strength 〉=0.3MPa, and elongation at break 〉=100%, the thermal conductivity to air is 0.03～0.04W/mK at normal temperatures.Because foaming system is stable, the poromerics of present method gained is fit to do large-scale foaming product, and as the foam sheet of wide cut, its width can reach more than the 0.5m.This poromerics is applicable to very extensive fields.
Simple, the easy handling of the method for preparing millipore polyethene material of the present invention is applicable to the kinds of processes of polyethylene foam.
Further describe the present invention below in conjunction with embodiment, scope of the present invention is not subjected to the restriction of these embodiment.Scope of the present invention proposes in claims.
Accompanying drawing 1 is embodiment 8 gained sample electromicroscopic photographs, and magnification is about 20 times.
Accompanying drawing 2 is the kinds of processes schematic flow sheet of the polyethylene foam of use present method.
Embodiment 1
(english abbreviation is the LDPE place of production: Shandong, the Shandong trade mark: 2101TN00) pass through the high-speed mixer uniform mixing with processing aid with new LDPE (film grade), by twin screw extruder melt blending, crosslinked extrused and through port mould formation sheet material, blending temperature is 170 ℃ then.With sheet material foamable on hot drying tunnel, blowing temperature is 220 ℃, and foamed time is 7 minutes.Cooling afterwards obtains foam sheet.Processing aid is Cellmic C 121 (AC), dicumyl peroxide (DCP), silicon-dioxide (SiO
2), white oil, decabromodiphenyl oxide and antimonous oxide, all can be commercially available and get.Prescription is 100 to see Table 1 in the matrix resin parts by weight.Properties of sample test result and testing standard see Table 2.
Embodiment 2～9
The processing condition of employed new LDPE (film grade) and experiment are with embodiment 1.Each component and the consumption of prescription see Table 1.Wherein processing aid comprises whipping agent: Cellmic C 121 (AC), Diisopropyl azodicarboxylate (AZDN); Linking agent: dicumyl peroxide (DCP), benzoyl peroxide (BPO); Nucleator: silicon-dioxide (SiO
2), talcum powder (1250 order); Liquid adjuvants: white oil, silicone oil; Fire retardant: decabromodiphenyl oxide, triphenylphosphate, antimonous oxide (Sb
2O
3), all can be commercially available and get.Be respectively with other resin of new LDPE (film grade) blend: high density polyethylene(HDPE) (english abbreviation is the HDPE place of production: the Shandong company trade mark: DMDA6158), linear low density of polyethylene (english abbreviation is the LLDPE place of production: the Canadian E.I.Du Pont Company trade mark: 2907), ethylene-ethyl acetate (english abbreviation is the EVA place of production: the du pont company trade mark: Elvax560) and ethylene-propylene rubber(EPR) (english abbreviation is the EPR place of production: Japan Synthetic Rubber Co. Ltd's trade mark: JSR EP57).Properties of sample test result and the testing standard of each embodiment see Table 2.
Comparative example 1
Except not with nucleator and the liquid adjuvants, all the other components, consumption and processing condition are all identical with embodiment 1.Prescription sees Table 1.In this comparative example blend extrude very difficult and can not moulding, can't carry out performance test.
Comparative example 2
Except whipping agent Cellmic C 121 consumption is reduced to 6 especially, all the other components, consumption and processing condition are all identical with embodiment 1.Prescription sees Table 1, and properties of sample test result and testing standard see Table 2.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | Comparative Examples 1 | Comparative Examples 2 | |
| ??LDPE | ????100 | ????100 | ????100 | ????90 | ????80 | ????92 | ????60 | ????80 | ????100 | ??100 | ??100 |
| ??HDPE | ????0 | ????0 | ????0 | ????0 | ????10 | ????0 | ????20 | ????0 | ????0 | ??0 | ??0 |
| ??LLDPE | ????0 | ????0 | ????0 | ????10 | ????0 | ????0 | ????10 | ????0 | ????0 | ??0 | ??0 |
| ??EVA | ????0 | ????0 | ????0 | ????0 | ????0 | ????8 | ????0 | ????20 | ????0 | ??0 | ??0 |
| ??EPR | ????0 | ????0 | ????0 | ????0 | ????12 | ????0 | ????10 | ????0 | ????0 | ??0 | ??0 |
| ??AC | ????20 | ????16 | ????24 | ????18 | ????20 | ????0 | ????0 | ????20 | ????20 | ??20 | ??6 |
| ??AZDN | ????0 | ????0 | ????0 | ????0 | ????0 | ????20 | ????20 | ????0 | ????0 | ??0 | ??0 |
| ??DCP | ????1 | ????0.8 | ????0 | ????0.7 | ????0 | ????0.8 | ????0.8 | ????0.8 | ????0.8 | ??1 | ??1 |
| ??BPO | ????0 | ????0 | ????0.8 | ????0 | ????1 | ????0 | ????0 | ????0 | ????0 | ??0 | ??0 |
| ??SiO 2 | ????1 | ????0 | ????0.5 | ????0 | ????1 | ????0.5 | ????1 | ????0 | ????0 | ??0 | ??1 |
| Talcum powder | ????0 | ????1 | ????0 | ????1.5 | ????0 | ????0 | ????0 | ????0.5 | ????1 | ??0 | ??0 |
| White oil | ????2 | ????1 | ????0 | ????0 | ????1 | ????0 | ????0 | ????0 | ????5 | ??0 | ??2 |
| Silicone oil | ????0 | ????0 | ????2 | ????1 | ????0 | ????1 | ????2 | ????1 | ????0 | ??0 | ??0 |
| Decabromodiphenyl oxide | ????15 | ????10 | ????0 | ????15 | ????0 | ????0 | ????0 | ????0 | ????0 | ??15 | ??15 |
| ??Sb2O3 | ????5 | ????5 | ????0 | ????0 | ????0 | ????5 | ????0 | ????0 | ????0 | ??5 | ??5 |
| Triphenylphosphate | ????0 | ????0 | ????0 | ????0 | ????0 | ????0 | ????0 | ????3 | ????0 | ??0 | ??0 |
Table 2
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | Comparative Examples 2 | Unit | Standard | ||
| Apparent density | ??38 | ??48 | ??24 | ??45 | ??22 | ??35 | ??32 | ??28 | ??30 | ??150 | ??kg/m 3 | ??GB ??6343- ??86 | |
| Area density | ??0.23 | ??0.27 | ??0.18 | ??0.26 | ??0.13 | ??0.22 | ??0.19 | ??0.17 | ??0.22 | ??0.30 | ??kg/m 2 | ??EN29 ??073- ??T1 | |
| Tensile strength | ??0.44 | ??0.65 | ??0.20 | ??0.65 | ??0.10 | ??0.32 | ??0.47 | ??0.40 | ??- | ???- | ??Mpa | ??GB ??10654 ??-89 | |
| Elongation at break | ??1.96 | ??210 | ??112 | ??200 | ??80 | ??112 | ??180 | ??190 | ??- | ????- | ??％ | ??GB ??10654 ??-89 | |
| Heat-resisting dimensional change | Horizontal | ??3.40 | ??3.43 | ??4.00 | ??3.53 | ??4.40 | ??3.50 | ??3.00 | ??3.90 | ??- | ????- | ??％ | ??DIN ??45113 ??9 |
| Vertical | ??0.50 | ??0.49 | ??0.99 | ??0.75 | ??1.40 | ??1.20 | ??1.62 | ??1.40 | ??- | ????- | ??％ | ||
| Combustionvelocity | ??85 | ??90 | ???- | ??92 | ???- | ??100 | ???- | ??86 | ??- | ????- | ??mm/ ??min | ??DIN ??45133 ??3 | |
| The aperture | ??0.33 | ??0.30 | ??0.40 | ??0.45 | ??0.55 | ??0.45 | ??0.55 | ??0.63 | ??- | ????- | ??mm | ??- | |
| Width | ??0.9 | ??0.5 | ??1.0 | ??0.9 | ??1.3 | ??1.3 | ??0.9 | ??1.0 | ??- | ????- | ??m | ??- | |
| Thickness | ??6 | ??10 | ??4 | ??8 | ??4 | ??8 | ??6 | ??4 | ??- | ????- | ??mm | ??- | |
Claims (18)
1. millipore polyethene material, the matrix resin that it is characterized in that described millipore polyethene material comprises the blend of new LDPE (film grade) or new LDPE (film grade) and other polymkeric substance, this kind millipore polyethene material is the obturator-type structure, mean pore size is 0.20～0.60mm, and the apparent density of millipore polyethene material is 20～100kg/m
3, area density is 0.1～0.4kg/m
2, material thickness is 1～10mm.
2. millipore polyethene material according to claim 1, it is characterized in that described matrix resin is the blend of new LDPE (film grade) and following at least a material: high density polyethylene(HDPE), linear low density of polyethylene, polyhutadiene, ethylene-ethyl acetate copolymer, second third copolymer or ethylene-propylene terpolymer, wherein the new LDPE (film grade) weight ratio that accounts for blend is (60～95): 100.
3. millipore polyethene material according to claim 1 is characterized in that the weight ratio that new LDPE (film grade) in the blend of described new LDPE (film grade) and other polymkeric substance accounts for blend is (80～90): 100.
4. millipore polyethene material according to claim 1, the apparent density that it is characterized in that this profit millipore polyethene material is 25～35kg/m
3
5. millipore polyethene material according to claim 1 is characterized in that the tensile strength 〉=0.3MPa of this kind millipore polyethene material, elongation at break 〉=100%, and the thermal conductivity to air is 0.03～0.04W/m.K at normal temperatures.
6. millipore polyethene material according to claim 1 is characterized in that this kind millipore polyethene material is that fabric width 〉=0.5m, thickness are the sheet material of 4～10mm.
7. according to the preparation method of each described millipore polyethene material of claim 1-6, crosslinked and chemical method foaming makes described millipore polyethene material to this preparation method by chemical method, may further comprise the steps:
(1) matrix resin is mixed with processing aid, processing aid comprises solid state chemistry whipping agent, linking agent, nucleator and liquid adjuvants, and prescription is counted with parts by weight:
Matrix resin 100
Whipping agent 10～28
Linking agent 0.3～7
Nucleator 0.2～2
Liquid adjuvants 0.5～10
Wherein whipping agent is an azo-compound, and linking agent is a decomposition temperature at 110～170 ℃ organo-peroxide, and nucleator comprises the solid particulate of inorganic salts and metal oxide, and liquid adjuvants is low molecule straight chain hydrocarbon of liquid or the low molecule silicoorganic compound of liquid;
(2) with mixture blend, crosslinked aftershaping;
(3) with the section bar thermostatically heating, foaming obtains goods.
8. preparation method according to claim 7 is characterized in that blending temperature is 150～170 ℃ in the described blend step, and be 3～15 minutes heat-up time in the foamable step, and blowing temperature is 200～230 ℃.
9. preparation method according to claim 7 is characterized in that filling a prescription and counts with parts by weight:
Matrix resin 100
Whipping agent 15～22
Linking agent 0.5～5
Nucleator 0.5～1.5
Liquid adjuvants 1～5.
10. preparation method according to claim 7 is characterized in that whipping agent is Cellmic C 121 or Diisopropyl azodicarboxylate.
11. preparation method according to claim 7 is characterized in that linking agent is dicumyl peroxide or benzoyl peroxide.
12. preparation method according to claim 7 is characterized in that nucleator is silicon-dioxide, talcum powder, lime carbonate, zinc oxide or magnesium oxide.
13. preparation method according to claim 7 is characterized in that liquid adjuvants is white oil, whiteruss or silicone oil.
14. preparation method according to claim 7 is characterized in that described processing aid also includes fire retardant.
15. preparation method according to claim 14, it is characterized in that described fire retardant comprises at least a of phosphonium flame retardant or following fire retardant: halogen flame, antimonous oxide, the phosphonium flame retardant consumption counts 2～6 with parts by weight, the total consumption of halogen flame and antimonous oxide is 100 to count 3～25 with the matrix resin parts by weight, and weight ratio is 1: 3～1: 2 when antimonous oxide and halogen flame use jointly.
16. preparation method according to claim 15, it is characterized in that described phosphonium flame retardant comprises: trimethyl phosphite 99, triphenylphosphate, tricresyl phosphate (2,3-two chloropropyls) ester, tricresyl phosphate toluene bromide ester, red phosphorus or Tetrakis hydroxymethyl phosphonium chloride, described halogen flame comprises: decabromodiphenyl oxide, octa-BDE, hexabromobenzene, clorafin or perchloro-penta cyclodecane.
17. preparation method according to claim 16 is characterized in that described phosphonium flame retardant is a triphenylphosphate, described halogen flame is a decabromodiphenyl oxide.
18. preparation method according to claim 15 is characterized in that the total consumption of described halogen flame and antimonous oxide is 100 to count 8～15 with the matrix resin parts by weight.
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